title: Sensitive determination of polycyclic aromatic hydrocarbons in water samples using monolithic capillary solid-phase extraction and on-line thermal desorption prior to gas chromatography-mass spectrometry.
abstract: A methacrylate-based monolithic capillary column has been evaluated for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. For this purpose, the monolyte was in situ synthesized in a 6cm×0.32mm id fused-silica capillary. The microextraction unit was fitted to a micro-HPLC pump to pass 10mL of sample. The isolated pollutants were eluted by means of 10μL of methanol, the organic phase being directly collected in a specific interface that can be fitted to the injection port of the gas chromatograph without modification. The interface allows the on-line thermal desorption of the PAHs, avoiding the dilution and providing enough sensitivity to reach the legal limits established for these pollutants in the matrices selected. The limits of detection achieved for 10mL of water ranged between 2.8ng/L (indeno(1,2,3-cd)pyrene) and 11.5ng/L (acenaphthene) with acceptable precision (between 4.5 and 18.2% RSD). The method was applied to the determination of the selected PAHs in tap, river waters and sewage, being fluoranthene and pyrene detected in all of them at concentrations lower than the legal limits established for these compounds in the matrices assayed.
authors.affiliation: Department of Analytical Chemistry, Campus Rabanales, University of Córdoba, 14071 Córdoba, Spain.
authors.forename: Francisco
authors.initials: F
authors.lastname: Galán-Cano
authors.forename: Virginia
authors.initials: V
authors.lastname: Bernabé-Zafón
authors.forename: Rafael
authors.initials: R
authors.lastname: Lucena
authors.forename: Soledad
authors.initials: S
authors.lastname: Cárdenas
authors.forename: José Manuel
authors.initials: JM
authors.lastname: Herrero-Martínez
authors.forename: Guillermo
authors.initials: G
authors.lastname: Ramis-Ramos
authors.forename: Miguel
authors.initials: M
authors.lastname: Valcárcel
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D011084:Polycyclic Aromatic Hydrocarbons; D012722:Sewage; D014874:Water Pollutants, Chemical